ASTM D7633-2013(2018) 6875 Standard Test Method for Carbon Black&x2014 Carbon Content.pdf

1、Designation: D7633 13 (Reapproved 2018)Standard Test Method forCarbon BlackCarbon Content1This standard is issued under the fixed designation D7633; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A numbe

2、r in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the instrumental determinationof carbon content in a carbon black sample. Values obtainedrepresent the total carbon

3、content.1.2 The method is applicable to tread, carcass and specialtytype carbon blacks obtained from partial combustion or ther-mal decomposition processes, which typically contain 95 to100 % carbon.1.3 The results of these tests can be expressed as mass %carbon.1.4 The values stated in SI units are

4、 to be regarded asstandard. No other units of measurement are included in thisstandard.1.5 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety, health, and environm

5、ental practices and deter-mine the applicability of regulatory limitations prior to use.1.6 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards,

6、 Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D1799 Practice for Carbon BlackSampling PackagedShipmentsD1900 Practice for Carbon BlackSampling Bulk Ship-mentsD4483 Practice for Evaluating Prec

7、ision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustries3. Summary of Test Method3.1 In this test method, a sample is weighed in a combustionboat and the carbon content is determined by placing the boatin a tube furnace operating at 1350C in a stream of oxygenresulting i

8、n complete combustion. Carbon in the sample isoxidized to carbon dioxide. Moisture and particulates areremoved from the gas stream by traps filled with anhydrousmagnesium perchlorate. The gas stream is then passed througha cell in which carbon dioxide concentration is measured by aninfrared (IR) abs

9、orption detector at a precise wavelength in theIR spectrum.3.2 This test method is for use with commercially availablecarbon analyzers equipped to carry out the combustion andmeasurement operations automatically.3.3 The carbon analyzer must be calibrated using an appro-priate calibration standard (s

10、ee 6.4).4. Significance and Use4.1 The total carbon content of a carbon black is a require-ment for the calculation and reporting of carbon dioxideemissions. It can also be used in calculations to estimate yieldof the process.5. Apparatus5.1 Analytical Balance, or equivalent, capable of a weighingse

11、nsitivity of 1 mg or better resolution.5.2 Gravity Convection Drying Oven, capable of maintain-ing 125 6 5C.5.3 Measurement Apparatus, equipped to automaticallycombust the sample and measure carbon content.5.4 Combustion tube and boat made of a suitable materialsuch as mullite, porcelain or zircon.6

12、. Reagents6.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,1This test method is under the jurisdiction of

13、ASTM Committee D24 on CarbonBlack and is the direct responsibility of Subcommittee D24.66 on Environment,Health, and Safety.Current edition approved June 1, 2018. Published August 2018. Originallyapproved in 2010. Last previous edition approved in 2013 as D7633 13. DOI:10.1520/D7633-13R18.2For refer

14、enced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West

15、Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trad

16、e Organization Technical Barriers to Trade (TBT) Committee.1where such specifications are available.3Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.6.2 Magnesium Perchlorate

17、.6.3 Oxygen, high purity, 99.9 %.6.4 Calibration standard.47. Sampling7.1 Samples of candidate carbon blacks shall be taken inaccordance with Practice D1799 or D1900.8. Preparation of Apparatus8.1 Assemble the apparatus according to the manufacturersinstructions.8.2 Stabilize the furnace temperature

18、 at 1350 6 15C.8.3 Make a minimum of two determinations to condition theequipment or follow manufacturers recommendation to con-dition equipment prior to calibrating the instrument.9. Calibration9.1 Calibrate the instrument per manufacturers recommen-dation using a carbon calibration standard.9.2 Ad

19、justment of Response of Measurement SystemWeigh approximately 0.1 g of calibration standard or userecommended mass per manufacturer. Analyze the sample (seeSection 10). Repeat this procedure. Adjust instrument asrecommended by the manufacturer until the absence of drift isindicated.9.3 Calibration P

20、rocedureFollow the calibration proce-dure recommended by the manufacturer. Confirm the calibra-tion by analyzing a reference material of known carbonconcentration.4Reference standards should be similar to car-bon black with carbon content of approximately 95-100 %. Themeasured value should be within

21、 allowable limits of the knownvalue. If not, repeat the procedure. If acceptable results are notobtained refer to the manufacturers instructions for calibra-tion.10. Procedure10.1 Sample PreparationDry an adequate sample of thecarbon black for at least1hinagravity-convection oven set at125 6 5C, in

22、an open container of suitable dimensions, so thatthe depth of black is no more than 10 mm. Cool to roomtemperature in a desiccator before use.10.2 Stabilize and verify calibration of the analyzer (see 8.1through 9.3).10.3 Confirm the furnace temperature is 1350 6 15C.10.4 Weigh approximately 0.1 g o

23、f the sample or userecommended mass per manufacturer.10.5 Spread the sample in the combustion boat and recordthe sample weight.10.6 Initiate the analysis and place the sample in theinstrument using a boat puller or the auto-sampler mechanism.10.7 When the analysis is complete, the instrument shouldi

24、ndicate the carbon value. Refer to the manufacturers recom-mended procedure.11. Report11.1 The percent carbon value is obtained directly from theapparatus.11.2 Report results from individual determinations to thenearest 0.1 %.NOTE 1The most representative measurement of carbon content in acarbon bla

25、ck sample is an average value from multiple individualdeterminations. A good practice is to report a minimum of two individualdeterminations for a given sample.12. Precision and Bias512.1 These precision statements have been prepared inaccordance with Practice D4483. Refer to this practice fortermin

26、ology and other statistical details.12.2 The precision results in this precision and bias sectiongive an estimate of the precision of this test method with thematerials used in the particular interlaboratory program de-scribed below. The precision parameters should not be used foracceptance or rejec

27、tion testing of any group of materialswithout documentation that they are applicable to those par-ticular materials and the specific testing protocols of the testmethod. Any appropriate value may be used from Table 1 forthe High Temperature Combustion Method. An alternatemethod for carbon content, C

28、HN, was included in the inter-laboratory program used to generate this precision statementsince a number labs use this instrumental method. Precisiondata specific to the CHN method is found in Table 2.12.3 A type 1 inter-laboratory precision program was con-ducted. Both repeatability and reproducibi

29、lity represent short-term (daily) testing conditions. The testing was performed ineach laboratory performing the test twice on each of two days(total of four tests). A test result is the value obtained from asingle determination. Acceptable difference values were notmeasured.12.4 The results of the

30、precision calculations for this test aregiven in Table 1. The materials are arranged in ascending“mean level” order.12.5 RepeatabilityThe pooled absolute repeatability, r, ofthis test has been established as 0.74 %. Any other value inTable 1 may be used as an estimate of repeatability, asappropriate

31、. The difference between two single test results (ordeterminations) found on identical test material under therepeatability conditions prescribed for this test will exceed the3“Reagent Chemicals,” American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on

32、the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K. and the United States Pharmacopeia andNational Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.4Purified carbon standards are typically

33、 available from the instrument manufac-turer.5A research report is pending.D7633 13 (2018)2repeatability on an average of not more than once in 20 casesin the normal and correct operation of the method. Two singletest results that differ by more than the appropriate value fromTable 1 must be suspect

34、ed of being from different populationsand some appropriate action taken.NOTE 2Appropriate action may be an investigation of the test methodprocedure or apparatus for faulty operation or the declaration of asignificant difference in the two materials, samples, etc., which generatedthe two test result

35、s.12.6 ReproducibilityThe pooled absolute reproducibility,R, of this test has been established as 2.68 %. Any other valuein Table 1 may be used as an estimate of reproducibility, asappropriate. The difference between two single and indepen-dent test results found by operators working under the pre-s

36、cribed reproducibility conditions in different laboratories onidentical test material will exceed the reproducibility on anaverage of not more than once in 20 cases in the normal andcorrect operation of the method. Two single test resultsproduced in different laboratories that differ by more than th

37、eappropriate value from Table 1 must be suspected of beingfrom different populations and some appropriate investigativeaction taken.12.7 BiasIn test method terminology, bias is the differencebetween an average test value and the reference (true) testproperty value. Reference values do not exist for

38、this testmethod since the value or level of the test property isexclusively defined by the test method. Bias, therefore, cannotbe determined.13. Keywords13.1 carbon black; carbon content; combustion; carbondioxide emissionsASTM International takes no position respecting the validity of any patent ri

39、ghts asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at an

40、y time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments w

41、ill receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by A

42、STM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail);

43、or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ 1 Precision Parameters for Test Method D7633, Type 1 Precision, High Temperature Combustio

44、n, Carbon Content of CarbonBlackUnitsPercentMaterialNumber ofLaboratoriesMean Level Sr r (r) SR R (R)1. AR-2029A3 100.03 0.115 0.33 0.33 0.115 0.33 0.332. SRB8G (N990) 4 99.62 0.238 0.67 0.68 0.388 1.10 1.103. SRB8E (N660) 4 98.32 0.393 1.11 1.13 0.932 2.64 2.684. Specialty 4 91.63 0.224 0.64 0.69 1

45、.594 4.51 4.92Average 97.40Pooled Values 0.262 0.74 0.76 0.945 2.68 2.75AAR-2029 is a high purity graphite (99.998 % C) certified reference material (CRM). This CRM was used as a calibration standard for the High Temperature CombustionMethod within the inter-laboratory program.The sole source of sup

46、ply of the CRM known to the committee at this time is Alpha Resources, Inc. If you are aware of alternative suppliers, please providethisinformation to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee,1which you may

47、attend.TABLE 2 Precision Parameters for Test Method D7633, Type 1 Precision, CHN, Carbon Content of Carbon BlackUnitsPercentMaterialNumber ofLaboratoriesMean Level Sr r (r) SR R (R)1. AR-2029 7 99.59 0.448 1.27 1.27 0.726 2.06 2.062. SRB8G (N990) 7 99.10 0.207 0.59 0.59 0.615 1.74 1.763. SRB8E (N660) 7 97.39 0.254 0.72 0.74 0.434 1.23 1.264. Specialty 7 88.79 0.252 0.71 0.80 2.823 7.99 9.00Average 96.22Pooled Values 0.305 0.86 0.90 1.505 4.26 4.43D7633 13 (2018)3